Hydrochloric Acid → Hydrochloric Acid

HRID 1395303ノート

反応式

HRID 1395303 の反応式
C1(N2CCNCC2)C=CC=CC=1.C([O:20][C:21]1[CH:41]=[CH:40][C:24]([O:25][CH2:26][CH2:27][N:28]2[CH2:33][CH2:32][N:31]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)[CH2:30][CH2:29]2)=[CH:23][CH:22]=1)C1C=CC=CC=1.[ClH:42]>CCO>[OH:20][C:21]1[CH:22]=[CH:23][C:24]([O:25][CH2:26][CH2:27][N:28]2[CH2:29][CH2:30][N:31]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)[CH2:32][CH2:33]2)=[CH:40][CH:41]=1.[ClH:42]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 203407541-[2-(-4-Benzyloxyphenoxy)ethyl]-4-phenylpiperazine phenylpiperazine

生成物 2

HCID 313Hydrochloric AcidHCID 129411041-[2-(4-Hydroxyphenoxy)ethyl]-4-phenylpiperazine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

35.75 g of 1-[2-(-4-benzyloxyphenoxy)ethyl]-4-phenylpiperazine phenylpiperazine was added rapidly with stirring to 75 ml concentrated HCl and the mixture was heated on a steam bath for 15 minutes. During this time starting material dissolved and then a white crystalline solid began to form and eventually the reaction mixture almost solidified. The reaction was cooled to ~5° and then was diluted with 100 ml EtOH. The solids were filtered off and were washed in EtOH and ether to give 1-[2-(4-hydroxyphenoxy)ethyl]-4-phenylpiperazine as its monohydrochloride. The salt was dissolved in 150 ml hot MeOH and 50 ml H2O and was then treated with 25 ml triethylamine. Water was then added to the refluxing mixture just to the cloud point whereupon the product began to crystallize from solution. The mixture was chilled and the solids were collected by filtration to give the end product, mp 142°-143°.

後処理

  1. temperaturethe mixture was heated on a steam bath for 15 minutes
  2. dissolutiondissolved
  3. customto form
  4. temperatureThe reaction was cooled to ~5°
  5. filtrationThe solids were filtered off
  6. washwere washed in EtOH

出典と根拠

ORDレコード
ord-722f1ac77fb24264884eb1d4ddf61857
出典データセット
uspto-grants-1980_05
特許番号
US04202978

反応ノート

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